Process for making furfural resins



meme A r. 10,1928.

UNITED STATE JOHN r. 'rnIcxEY, or EvAN'sroN, sreNoas 'ro THE'QUAKER 'rroN or NEW JERSEY.

PATENT-I ore-ice.

i ocEss Eon MAKING FURF'UBAL EEsINs.

Ho Drawing. Application filed. May 26, 1924, Serial No. 715,816. Renewed- February 27,1928.

This invention pertains to methods or processes for making resinous materials from furane derivatives and more particularly relates to processes for making furfural resins.

It is the purpose of this invention to provide a rapid, inexpensive and eflicient process for making resinous mater alsfrom fuone of rane derivatives.- More specifically, the objects of this invention is to provide an efiicient catalyst for causing rapidresinificamay be readily tion of .furane derivatives. and particularly furfural.

A further object of this invention is to provide a catalyst for this purpose which removed from the material after the reaction has progressed to the desired extent. Catalysts which are fluid or in the form of solutions are often difiicult to use in practice particularly if it is desired to check the reaction at a partially completed also manifest itself by a slight resinificabe manifested by the-formation of stage.

Under properly controlled conditions certain reactions will take placein furane derivatives, formation of resinous materials. We have discovered that such reactions may be made to take place by at least threeLdifierent methods. First, furfural by itselfmaybe continuously heated for a long period of time and after several'months the reaction will small amounts of soft resinous material. Second, furfural may beallowed to stand without heating for a year or more in the presence of a suitable catalyst and the reaction will tion. Third, a furane derivative, such as furfural, may be heated in the presence of a catalyst and resinification will take place much more quickly than with the independent use of either heat or a-catalyst.

We have discovered that under properly controlled conditions various metals comprise very efiicient catalysts for use in the resinification of furane derivatives, such-as furfuralr Among the metals found to be efiective as catalysts. are iron, nickel. lead, magnesium, be preferably added to the furfural in the form of finelydivided particles, or in'the form of a precipitate of the metalen a porous inert material, although if the furfural is constantly agitated satisfactory catalytic efiects are obtainable by merely placing the producing a may be controlled either by the such as furfural, resulting in the.

temperatures between 163"170- zinc and tin. These metals may degrees 0 furfural in a container made of one of the above mentioned metals. While several met als have been enumerated above which serve efiectivelyas catalystsfor the reaction in furfural resin fronnfurfural, it is conceivable that many other metals will act in a similar manner and, therefore, the term metal catalyst for the reaction and the term metal that serves as a catalyst for the reaction refer. to those metals only which act in the nature of catalytic agents in producing a furfural resin from fur'fu The rate at which the reaction takes place form of catalyst used or by regulation of thetemperature. 1 Thus if furfural is continuously heated at a temperature of 100110 C. in the presence ofv iron, nickel or lead for several days. resinifi-cation is manifested by the formation of a thick jelly. However, in

order to secure a more rapid rate of reac heated under pressure for several hours at C. 1n the farmers, as:

ral.

presence of one of the above mentioned metallic catalysts; As soft viscous resin first forms which later chances to a semi-solid stage. The'resinin this form is fusible and is soluble in acetone and the like. but insoluble in water. Ifthe reaction is allowed to proceed to a conclusion. the fusible, soluble product istransformed into an insoluble. infusihle solid.

the reactionproceeds a In any case,.the character of the product may be easily controlled by merely removing the resinous material from contact with the metallic catal st. For example, if the catalvst is in the form of a metal container. itis merely necessary to remove the resinous b y from the container or if the catalyst isin the form of small particles, the resin may be separated therefrom by any suitable known mechanical process.

.By thus properly controlling the speed and extent of the reaction as above described,

we are able to secure a product of various stage at which the reaction is stopped. Furthermore, the resulting product formed by stopping the reaction at any particularintermediate stage maybe substantially perfconsistency. dependingupon the I manently retained at its existing consistency by the removal of the catalyst.

Since the reaction is readily controlled in. accordance with our invention and may be arrested at any stage in the resinificationof the furane derivative, the resulting resms are adaptable to the various well known uses 'ployed the term furane derivative.

of the natural and synthetic resins.

Throughout this application we haveiemto be understood, however, that by this term is meant a chemical compound containing no I and substitutions of equivalents may be madewithoutdeparting fromthe scope and prin-,

other ring nucleus but 'the furane ring, as distinguished from a furane compound which is a chemical compound containing another ring nucleus or other ring nuclei besides the furane ring.

' It will be understood that various changes ciple of theinvention set forth or intended to beset forth in theappended claims. Having thus described our invention, what we claim as new and desire to secure by Letters Patent of the United States, is: 1. The process of making a furfural resin which comprises heating furfural in the presence of a metal that serves as a catalyst for this reaction.

2. The process of obtaining a resinous substance which comprises treating furfural' resin.

The process of obtaining a furfural resin which comprises submitting furfural with a metal that serves as a catalyst for the f reaction to such temperature and ressure as to produce afusible soluble resin.

5. 'The process 'of obtaining a .furfural resin which comprises heating furfural catalyst ,for the reaction to. a temperature above the atmospheric boiling point of furfural until a fumble soluble resln is formed.

6. The process of obtaining a furfural resin which comprises heating furfural with 4 a catalyst embodying at leastone metal .under pressure with a metal serving as a that serves'as a catalyst for the reaction to such a temperature and under slfch'pres sure that a non-gelatinous resinous reaction I product is produced.

In witness whereof, we have hereunto subscribed our names.

CARL s. MINER.

JOHN TRICKEY. 

